HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 86748237, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Dibenzo(c,f)pyrazino(1,2-a)azepine, 1,2,3,4,10,14b-hexahydro-, (14bS)- | HCID 153934 | — |
| Reactant | Ethyl 2-(2-chloroethoxy)acetate | HCID 10964894 | — |
| Catalyst | Sodium Iodide | HCID 5238 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 86748237 | HCID 86748237 | 91% |
Reaction Steps
32.48 g of (S)-1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1,2-a]azepine (prepared as described in Preparation 3), 22.7 g of ethyl 2-chloroethoxyacetate, 48.9 g of sodium carbonate and 0.79 g of sodium iodide were added to 340 ml of 4-methyl-2-pentanone, and the mixture was heated under reflux for 16 hours. At the end of this time, it was cooled to room temperature and was filtered using a Celite filter aid, and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was subjected to column chromatography through silica gel eluted with a 1:1 by volume mixture of ethyl acetate and hexane, to give 44.85 g (yield 91%) of the title compound as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05476848 |
| Source dataset | uspto-grants-1995_12 |
| ORD ID | ord-5ebd3e085f5e4c7cb4cc16e9a4c022fb |
| Source note | uspto-grants-1995_12 |